CN101787213A - Calcium sulfate whisker-modified silicon rubber composite material and preparation method thereof - Google Patents
Calcium sulfate whisker-modified silicon rubber composite material and preparation method thereof Download PDFInfo
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- CN101787213A CN101787213A CN 201010136248 CN201010136248A CN101787213A CN 101787213 A CN101787213 A CN 101787213A CN 201010136248 CN201010136248 CN 201010136248 CN 201010136248 A CN201010136248 A CN 201010136248A CN 101787213 A CN101787213 A CN 101787213A
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Abstract
The invention discloses a calcium sulfate whisker-modified silicon rubber composite material and a preparation method thereof. The composite material comprises the following components in part by weight: a component A 98-100, a component B 2-5, a catalyst 0.1-0.2, calcium sulfate whisker 5-15 and silane coupling agent 0.05-0.45, wherein the component A is dihydroxy polydimethylsiloxane; the component B is tetraethoxysilane; and the catalyst is dibutyltin dilaurate. The cheap organically modifying calcium sulfate whisker used as a reinforcing material of the silicon rubber greatly improves the chemical reaction contact area and activity of the composite material. The product has improved tensile strength, elongation at break, thermal stability and the like and a promoting application prospect.
Description
Technical field
The present invention relates to a kind of modified silicon rubber matrix material and preparation method thereof.
Background technology
Silicon rubber has excellent thermotolerance, winter hardiness and electrical insulation capability, is widely used in electrical isolation goods and sealing article etc.Silicon rubber can be made a lot of moldingss, as various O type circles, pad, leather cup, oil sealing, valve, vibroshock and diaphragm etc.Because silicon rubber has physiology inertia, nontoxic, does not have adhesive capacity with other materials, and can stand repeatedly the characteristics of retort sterilization, is widely used in health care and foodstuffs industry aspect, as artificial heart valve, artificial larynx, artificial blood vessel, nipple and medicine bottle stopper etc.Coating, sealing as various electron tubes or electrical element have protection against the tide, keep away dirt, the shockproof and effect of improving electrical property.
The method that now more successfully prepares high-strength silicone rubber has: 1. adopt the white carbon black of handling, for example with 4 of hexamethyldisilazane processing
#Thermal silica, promptly high anti-tear white carbon black (or claiming high-reinforcement white carbon black), tear strength can reach 40~50kN/m.2. the low relative molecular mass polysiloxane (being commonly called as C glue) that adds high-vinyl-content in vinylsiloxane rubber is with 4
#White carbon black is that strengthening agent, silazane are constitution controller, tear strength can be brought up to 50~60kN/m.
Silicon rubber mainly uses thermal silica to strengthen, but this white carbon black price is more expensive, and homemade price is ten thousand yuan/ton of 6-10, and import price is ten thousand yuan/ton of 10-30; And because its particle diameter very little (20-100nm), easily assemble agglomeratingly, and be difficult for being dispersed in the rubber, also be inhaled into human body during operation easily, very big to the healthy influence of operator, easily cause " silicosis ".
Summary of the invention
The purpose of this invention is to provide a kind of calcium sulfate whisker-modified silicon rubber composite material and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
The component and the weight part of calcium sulfate whisker-modified silicon rubber composite material of the present invention are:
98~100 parts of first components
2~5 parts of second components
0.1~0.2 part of catalyzer
5~15 parts of calcium sulfate whiskers
0.05~0.45 part of silane coupling agent
The first component is a dialkyl polydimethylsiloxane, can adopt business-like product, and the trade mark of producing as blue star organosilicon (Shanghai) Co., Ltd. is the product of PC-2;
Component B is a tetraethoxy, can adopt business-like product, and the trade mark of producing as blue star organosilicon (Shanghai) Co., Ltd. is the product of PC-2;
Catalyzer is a dibutyl tin laurate;
Described calcium sulfate whisker is the fibrous single crystal of anhydrous calciumsulphate, and the white loose spicule has perfect structure, complete profile, specific cross section, stable size, and its average aspect ratio is generally 20~50 μ m.Have fineness, the flock of granulated filler length-to-diameter ratio, high temperature resistant, resistance to acids and bases, resist chemical, good toughness, electrical insulating property is good, intensity is high, easily carry out surface treatment, can homodisperse, the pH value is near neutral.Can adopt commercially produced product, the trade mark that provides cloudlike peak group is the product of JX-B;
The preferred aminopropyl triethoxysilane of described silane coupling agent, γ-glycidyl ether oxygen propyl trimethoxy silicane or γ-(methacryloxypropyl) propyl trimethoxy silicane, for example the trade mark of Shanghai boiling point chemical industry company limited production is KH550, KH560, or the product of KH570;
The preparation method of silicon rubber of the present invention/modified crystal whiskers calcium sulfate composite material comprises the steps:
(1) with calcium sulfate whisker and silane coupling agent and dispersant, 20~30 ℃ were stirred 30~50 minutes, were heated to 60~80 ℃, stirred 30~50 minutes, took out, and drying obtains modified crystal whiskers calcium sulfate;
Described dispersion agent is the aqueous ethanolic solution of weight concentration 40~60%;
Described silane coupling agent consumption is 1~3% of a calcium sulfate whisker weight consumption;
The weight ratio of dispersion agent and calcium sulfate whisker is: dispersion agent: calcium sulfate whisker=1: 1~2;
(2) calcium sulfate whisker after the modification is joined in the first component, 30~40 ℃ were stirred 10~30 minutes, added second component and catalyzer again, and 60~80 ℃ were stirred 20~40 minutes, the room temperature vacuum outgas promptly obtains described calcium sulfate whisker-modified silicon rubber composite material.
The present invention adopts the supporting material of low-cost organically-modified calcium sulfate whisker as silicon rubber, because calcium sulfate whisker is dispersed in after modification in the silicon rubber matrix, increase the contact surface and the activity of its chemical reaction greatly, after using modified crystal whiskers calcium sulfate, the tensile strength of product, elongation at break, thermal stabilities etc. all are improved, can give other reinforcing filler of the many employings of material unapproachable premium properties, processing characteristics is good, preparation technology is economical and practical, the physical and mechanical property excellence, these characteristics are significant to the practicability of silicon rubber/modified crystal whiskers calcium sulfate composite material, and its application prospect is very wide.
Embodiment
Press GB/T 1701-2001 and " nano composite polymer/laminated silicate material theory and practice " (QiZongNeng, Shang Wenyu writes, Chemical Industry Press, 2002) thermogravimetry, the mechanical property of test silicon rubber and matrix material thereof and the thermal weight loss core temperature of regulation.
Comparative Examples 1
2 gram second component tetraethoxys and 0.1 gram catalyzer dibutyl tin laurate are joined in the 98 gram first component dialkyl polydimethylsiloxanes, 30 ℃ were stirred 30 minutes, and vacuum outgas is poured in the Teflon mould then, place 24h under the room temperature, get silastic material.
The tensile strength of silastic material, elongation at break and thermal weight loss core temperature see Table 1.
Embodiment 1
100 gram calcium sulfate whiskers and 1 gram silane coupling agent are infiltrated in the aqueous ethanolic solution of 100 weight concentrations 40% that restrain, and 30 ℃ were stirred 30 minutes, were heated to 80 ℃, stirred 30 minutes, took out, and drying obtains modified crystal whiskers calcium sulfate.
The trade mark that silane coupling agent adopts Shanghai boiling point chemical industry company limited to produce is the product of KH550, and chemical name is an aminopropyl triethoxysilane.
Calcium sulfate whisker after the 5 gram modifications is joined in the 98 gram first component dialkyl polydimethylsiloxanes, 40 ℃ were stirred 10 minutes, add 2 gram second component tetraethoxy linking agents and 0.1 gram catalyzer dibutyl tin laurate again, 60 ℃ were stirred 40 minutes, the room temperature vacuum outgas, pour into then in the Teflon mould, promptly obtain matrix material of the present invention.
The tensile strength of silicon rubber/modified crystal whiskers calcium sulfate composite material, elongation at break and thermal weight loss core temperature see Table 1.
Embodiment 2
The weight concentrations that 100 gram calcium sulfate whiskers and 2 gram silane coupling agents are infiltrated on 150 grams are in 50% aqueous ethanolic solution, and 25 ℃ were stirred 40 minutes, were heated to 70 ℃, stirred 40 minutes, took out drying, acquisition modified crystal whiskers calcium sulfate.
The trade mark that silane coupling agent adopts Shanghai boiling point chemical industry company limited to produce is the product of KH560, and chemical name is γ-glycidyl ether oxygen propyl trimethoxy silicane.
Calcium sulfate whisker after the 10 gram modifications is joined in the 99 gram first component dialkyl polydimethylsiloxanes, 35 ℃ were stirred 20 minutes, add 3 gram second component tetraethoxy linking agents and 0.15 gram catalyzer dibutyl tin laurate again, 70 ℃ were stirred 30 minutes, the room temperature vacuum outgas, pour into then in the Teflon mould, promptly obtain described matrix material.
The tensile strength of silicon rubber/modified crystal whiskers calcium sulfate composite material, elongation at break and thermal weight loss core temperature see Table 1.
Embodiment 3
100 gram calcium sulfate whiskers and 3 gram silane coupling agents are infiltrated in weight concentration 60% aqueous ethanolic solution of 200 grams, and 20 ℃ were stirred 50 minutes, were heated to 60 ℃, stirred 50 minutes, took out, and drying obtains modified crystal whiskers calcium sulfate.
The trade mark that silane coupling agent adopts Shanghai boiling point chemical industry company limited to produce is the product of KH570, and chemical name is γ-(methacryloxypropyl) propyl trimethoxy silicane.
Calcium sulfate whisker after the 15 gram modifications is joined in the 100 gram first component dialkyl polydimethylsiloxanes, 30 ℃ were stirred 30 minutes, add 5 gram second component tetraethoxy linking agents and 0.2 gram catalyzer dibutyl tin laurate again, 80 ℃ were stirred 20 minutes, the room temperature vacuum outgas, pour into then in the Teflon mould, promptly obtain described matrix material.
The tensile strength of silicon rubber/modified crystal whiskers calcium sulfate composite material, elongation at break and thermal weight loss core temperature see Table 1.
Table 1
Embodiment | Tensile strength/MPa | Elongation at break/% | The thermal weight loss core temperature/℃ |
Comparative Examples 1 | ??4.2 | ??210 | ??480 |
Embodiment 1 | ??4.5 | ??280 | ??505 |
Embodiment 2 | ??5.5 | ??350 | ??512 |
Embodiment 3 | ??4.9 | ??270 | ??508 |
Claims (4)
1. calcium sulfate whisker-modified silicon rubber composite material is characterized in that, component and weight part are:
98~100 parts of first components
2~5 parts of second components
0.1~0.2 part of catalyzer
5~15 parts of calcium sulfate whiskers
0.05~0.45 part of silane coupling agent
The first component is a dialkyl polydimethylsiloxane, and component B is a tetraethoxy, and catalyzer is a dibutyl tin laurate.
2. calcium sulfate whisker-modified silicon rubber composite material according to claim 1 is characterized in that, described calcium sulfate whisker average aspect ratio is 20~50 μ m.
3. calcium sulfate whisker-modified silicon rubber composite material according to claim 1 is characterized in that, described silane coupling agent is KH550, KH560 or KH570.
4. according to the preparation method of claim 1,2 or 3 described calcium sulfate whisker-modified silicon rubber composite materials, comprise the steps:
(1) with calcium sulfate whisker and silane coupling agent and dispersant, stir, be heated to 60~80 ℃, to take out, drying obtains modified crystal whiskers calcium sulfate;
Described dispersion agent is the aqueous ethanolic solution of weight concentration 40~60%;
Described silane coupling agent consumption is 1~3% of a calcium sulfate whisker weight consumption;
The weight ratio of dispersion agent and calcium sulfate whisker is: dispersion agent: calcium sulfate whisker=1: 1~2;
(2) calcium sulfate whisker after the modification is joined in the first component, stir, add second component and catalyzer again, stir, vacuum outgas promptly obtains described calcium sulfate whisker-modified silicon rubber composite material.
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Cited By (7)
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CN102250473A (en) * | 2011-06-16 | 2011-11-23 | 刘立文 | Modified cable coating composite material and preparation method thereof |
CN102936413A (en) * | 2012-10-31 | 2013-02-20 | 浙江优特格尔医疗用品有限公司 | Silica gel catheter sacculus with high tear strength and preparation method thereof |
CN105440690A (en) * | 2015-12-22 | 2016-03-30 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | 3D printer base material based on bulrush modification, and preparation method thereof |
CN106604969A (en) * | 2015-01-28 | 2017-04-26 | 瓦克化学股份公司 | Organopolysiloxane compositions which can be crosslinked by means of condensation reaction |
CN107343966A (en) * | 2017-05-31 | 2017-11-14 | 苏州蔻美新材料有限公司 | A kind of preparation method of artificial heart nano meter biomaterial |
CN109337112A (en) * | 2018-09-14 | 2019-02-15 | 晋江瑞碧科技有限公司 | Calcium sulfate crystal whiskers/melamine resin hollow ball material preparation method and its usage |
CN116410629A (en) * | 2022-01-05 | 2023-07-11 | 中国科学院青海盐湖研究所 | Super-hydrophobic powder material and preparation method and application thereof |
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CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
CN101671848A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of high length-diameter ratio anhydrous calcium sulfate whisker |
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JP2005350569A (en) * | 2004-06-10 | 2005-12-22 | Ntn Corp | Sliding material |
CN1908068A (en) * | 2006-08-14 | 2007-02-07 | 上海工程技术大学 | Heat-vulcanized silicone rubber containing nano montmorillonite and preparation method thereof |
CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
CN101671848A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of high length-diameter ratio anhydrous calcium sulfate whisker |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102250473A (en) * | 2011-06-16 | 2011-11-23 | 刘立文 | Modified cable coating composite material and preparation method thereof |
CN102250473B (en) * | 2011-06-16 | 2012-07-25 | 刘立文 | Modified cable coating composite material and preparation method thereof |
CN102936413A (en) * | 2012-10-31 | 2013-02-20 | 浙江优特格尔医疗用品有限公司 | Silica gel catheter sacculus with high tear strength and preparation method thereof |
CN106604969A (en) * | 2015-01-28 | 2017-04-26 | 瓦克化学股份公司 | Organopolysiloxane compositions which can be crosslinked by means of condensation reaction |
CN106604969B (en) * | 2015-01-28 | 2019-10-22 | 瓦克化学股份公司 | The organopolysiloxane composition that can be crosslinked by condensation reaction |
CN105440690A (en) * | 2015-12-22 | 2016-03-30 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | 3D printer base material based on bulrush modification, and preparation method thereof |
CN107343966A (en) * | 2017-05-31 | 2017-11-14 | 苏州蔻美新材料有限公司 | A kind of preparation method of artificial heart nano meter biomaterial |
CN109337112A (en) * | 2018-09-14 | 2019-02-15 | 晋江瑞碧科技有限公司 | Calcium sulfate crystal whiskers/melamine resin hollow ball material preparation method and its usage |
CN109337112B (en) * | 2018-09-14 | 2021-06-04 | 晋江瑞碧科技有限公司 | Preparation method and application of calcium sulfate whisker/melamine resin hollow sphere material |
CN116410629A (en) * | 2022-01-05 | 2023-07-11 | 中国科学院青海盐湖研究所 | Super-hydrophobic powder material and preparation method and application thereof |
CN116410629B (en) * | 2022-01-05 | 2024-02-27 | 中国科学院青海盐湖研究所 | Super-hydrophobic powder material and preparation method and application thereof |
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